EP1766102B1 - Verfahren zur herstellung hochfester und ermüdungsfester aluminiumlegierungsprodukte - Google Patents

Verfahren zur herstellung hochfester und ermüdungsfester aluminiumlegierungsprodukte Download PDF

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EP1766102B1
EP1766102B1 EP05778801A EP05778801A EP1766102B1 EP 1766102 B1 EP1766102 B1 EP 1766102B1 EP 05778801 A EP05778801 A EP 05778801A EP 05778801 A EP05778801 A EP 05778801A EP 1766102 B1 EP1766102 B1 EP 1766102B1
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Prior art keywords
alloy
barium
aluminium
type
worked
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French (fr)
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EP1766102A1 (de
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Emmanuelle Sarrazin
Philippe Jarry
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Constellium Issoire SAS
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Alcan Rhenalu SAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/10—Alloys based on aluminium with zinc as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/14—Alloys based on aluminium with copper as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C22C21/16—Alloys based on aluminium with copper as the next major constituent with magnesium

Definitions

  • the invention relates to a new manufacturing process for rolled, spun or forged products made of high tenacity and high fatigue strength aluminum alloy, especially Al-Zn-Cu-Mg type alloy, and products obtained by this method, including structural elements made from such products and intended for the construction of aircraft. It is based on the introduction of barium in an aluminum-based liquid alloy.
  • type 7xxx alloys are typically used for the wing structure elements. These elements must have high mechanical strength, good toughness and good resistance to fatigue. Any new opportunity to improve one of these property groups without degrading others would be welcome.
  • the iron and silicon elements form with the aluminum virtually insoluble intermetallic phases, such as Al 7 Cu 2 Fe, Al 6 (Fe x Mn 1-x ) (with 0 ⁇ x ⁇ 1), Al 12 Fe 3 Si, Al 9 Fe 2 Si 2 , Mg 2 Si.
  • these phases are more harmful than when they are small.
  • the possibilities of acting on their size during casting through the physical parameters (especially the rate of solidification) are unfortunately quite limited.
  • the patent FR 1 507 664 (Metallgesellschaft Aktiengesellschaft) notes that in Al-Si casting alloys with Si content between 5 and 14%, the addition of strontium and / or barium (Ba) at a rate of 0.001 to 2% leads to obtaining a fine eutectic structure; this effect is reinforced by the simultaneous addition of beryllium (Be).
  • the patent EP 1 230 409 B1 (RUAG Components) teaches that the addition of barium (between 0.1 and 0.8%) to aluminum alloys with a silicon content of at least 5% improves their ability to form thixotropically.
  • the patent GB 596.178 (Tennyson Fraser Bradbury) describes the addition of the Na, K, Ba and / or P elements at a maximum total content of 0.15% to an aluminum alloy containing Cu 5.00 - 9.50 %, Zr, Ni, Ce 0.05 - 1.00 in total, Si 0.02 - 0.40%, Fe 0.02 - 0.50%, Zn 0.00 - 0.25%. It is a casting alloy for pistons. Neither the function nor the mode of introduction of barium are specified.
  • the patent US 4,631,172 discloses an aluminum alloy used as a sacrificial anode containing 3.2% Zn, 1.5% magnesium, 0.02% indium, 0.01% d tin and / or calcium and barium, the latter in a content of between 0.002% and 1.0%.
  • Another composition contains Zn 2.5%, Mg 2.5%, In 0.02%, Ca and / or Ba 0.005 - 1.0%, Si 0.004 - 1.0%.
  • the addition of calcium and / or barium increases the current density and ensures uniform wear of the sacrificial anode.
  • the patent application JP 61 096052 A discloses an aluminum alloy sacrificial anode of composition Zn 1 - 10%, Mg 0.1 - 6%, In 0.01 - 0.04%, Sn 0.005 - 0.15%, Si 0.09 - 1%, Ca and / or Ba 0.005 - 0.45%.
  • CH 328 148 discloses the introduction of a barium hydride in a zinc-aluminum alloy with at least 40% zinc.
  • the patent RU 2 184 167 discloses an aluminum-based alloy for structural application in aeronautical construction of composition Cu 3.0 - 3.8%, Li 1.4 - 1.7%, Zr 0.0001 - 0 , 04%, Sc 0.16 - 0.35%, Fe 0.01 - 0.5%, Mg 0.01 - 0.7, Mn 0.05 - 0.5%, Ba 0.001 - 0.2% , Ga 0.001 - 0.08%, Sb 0.00001 - 0.001%.
  • the patent SU 1,678,080 discloses an aluminum-based alloy of composition Cu 5.0 - 5.5%, Cr 0.1 - 0.4%, Mn 0.2 - 0.6%, Zr 0 , 1 - 0.4%, Ti 0.1 - 0.4%, Cd 0.05 - 0.25%, Sr or Ba 0.01 - 0.1%.
  • the subject of the invention is a process defined in claim 1 for manufacturing wrought products made of aluminum alloy of Al-Cu-Mg or Al-Zn-Cu-Mg type with high tenacity and fatigue resistance, including casting. of a raw form (such as a spinning billet, forge billet or a rolling plate) and the hot deformation of said raw form, said method being characterized in that 0.005 is introduced into said alloy, and 0.1% barium.
  • a raw form such as a spinning billet, forge billet or a rolling plate
  • the invention also relates to a structural element for aircraft construction, manufactured from a rolled product, spun or forged alloy Al-Cu-Mg or Al-Zn-Cu-Mg which contains between 0.005 and 0 , 1% of barium as defined in claims 8, 9 and 10.
  • a product or structural element obtainable by the method according to the present invention, can be used advantageously in applications that require high tenacity and / or a high resistance to fatigue, such as extrados or intrados (wing skin) wing elements, stiffeners, longitudinal members, or ribs, or bulkhead elements (bulkheads).
  • the static mechanical characteristics ie the breaking strength R m , the yield stress R p0,2 , and the elongation at break A, are determined by a tensile test according to EN 10002-1 standard, the location and direction of specimen collection being defined in EN 485-1.
  • the fatigue strength is determined by a test according to ASTM E 466, the fatigue crack propagation rate (so-called da / dn test) according to ASTM E 647, and the critical stress intensity factor Kc, K CO or K App according to ASTM E 561.
  • the term "spun product” includes so-called “stretched” products, that is products that are made by spinning followed by stretching.
  • wrought product a product having undergone a deformation operation after its solidification
  • this deformation operation may be, without this list being exhaustive, rolling, forging, spinning, drawing and drawing.
  • structural element or “structural element” of a mechanical construction a mechanical part whose failure is likely to endanger the security of the said construction, its users, its users or others.
  • these structural elements include the elements that make up the fuselage (such as fuselage skin (fuselage skin in English), stiffeners or stringers, bulkheads, fuselage (circumferential frames), wings (such as wing skin), stiffeners (stiffeners), ribs (ribs) and spars) and empennage including horizontal stabilizers and vertical stabilizers horizontal or vertical stabilizers, as well as floor beams, seat tracks and doors.
  • integral structure refers to the structure of a portion of an aircraft that has been designed to provide as much continuity as possible over as large a dimension as possible to reduce the number of assembly points mechanical.
  • An integral structure can be manufactured either by machining in the mass, or by using shaped parts obtained for example by spinning, forging or molding, or by welding structural elements made of weldable alloys. This gives structure elements of larger size and in one piece, without assembly or with a reduced number of assembly points compared to an assembled structure in which sheets, thin or strong depending on the destination of the element of structure (for example: fuselage element or wing element), are fixed, usually by riveting, on stiffeners and / or frames (which can be manufactured by machining from spun or rolled products).
  • the present invention is applicable to Al-Cu-Mg or Al-Zn-Cu-Mg structural hardening aluminum based alloys.
  • the invention applies to alloys of the Al-Cu-Mg type comprising between 3.5 and 5.5% of Cu and between 1 and 2% of Mg, it being understood that the content of iron and silicon must not exceed 0.30% for each of these elements.
  • These alloys may contain other alloying elements and impurities up to about 3% in total. Among these elements are manganese, lithium, zinc.
  • the alloy may also contain the usual additions of zirconium, titanium or chromium.
  • the process according to the invention can advantageously be applied to alloys conventionally used in aeronautical construction: 2024, 2024A, 2056, 2124, 2224, 2324, 2424, 2524 and their variants.
  • the so-called free-cutting alloys which include additions of Pb, Bi or Sb in order to obtain easy splitting chips such as 2004, 2005 and 2030 are excluded here.
  • the alloys of Al-Zn-Cu-Mg type to which the present invention is applied are the alloys comprising between 4 and 14% of zinc, and more particularly between 7 and 10.5% of zinc, between 1 and 3% of Cu, and more particularly between 1.4 and 2.5% of Cu, and between 1 and 3% of Mg, and more particularly between 1.7 and 2.8% of Mg, it being understood that the content of iron and silicon must not exceed 0.30% for each of these elements.
  • These alloys can contain other alloying elements and impurities up to 2% in total. Among these elements is manganese.
  • the alloy may also contain the usual additions of zirconium, titanium or chromium.
  • the process according to the invention can advantageously be applied to alloys of the 7xxx series, in particular to those conventionally used in aeronautical construction: 7010, 7050, 7055, 7056, 7150, 7040, 7075, 7175, 7475, 7049, 7149, 7249 , 7349, 7449 and their variants.
  • the method according to the invention comprises casting a raw form, such as a rolling plate, a spinning billet or a forge billet, by any known method. This raw form is then deformed hot, for example by rolling, spinning or forging.
  • the invention is not applicable to products produced by fast solidification, ie with a solidification rate typically greater than 600 ° C / min, which lead to a significantly different microstructure.
  • the process may comprise other stages of thermal or mechanical treatment, the more often homogenization, cold deformation, dissolution, artificial or natural aging, intermediate or final annealing.
  • the applicant has surprisingly found that the presence of a very small amount of barium partially neutralizes the detrimental effect of iron and silicon for certain properties, as will be explained below. This results in a morphological modification of the intermetallic phases, and in particular that of the intermetallic iron phases (Al-Cu-Fe type).
  • the intermetallic eutectic phases are fragmented ("sea urchin” or “broccoli” morphology, see figure 2 ) whereas without barium, they have a more extensive form (morphology of "petals”, “platelets” or “cabbage leaves", see figure 1 ).
  • These eutectic phases may be of Al-Fe-Cu type (in alloys with addition of barium) or Al-Fe-Si-Cu (in alloys without addition of barium). It is observed that in the presence of barium, silicon seems to disappear precipitates.
  • the properties of the product which are improved by the process according to the invention are in particular the tenacity, the fatigue strength, and the resistance to the propagation of cracks da / dn with a high stress intensity factor ⁇ K. This effect is particularly pronounced in a non-recrystallized structure.
  • an alloy of barium with silicon is added.
  • An alloy of Si (70%) - Ba (30%) is suitable; this product is commercially available.
  • the silicon content of the alloy can be between 50% and 90%.
  • Other alloys of the same type containing in addition iron up to a content of 20% are also applicable to the invention, the silicon content can then vary between 30% and 90% and the barium content can then vary between 10 and 40%.
  • barium is added in metallic form or, preferably, in the form of an intermetallic compound or alloy with one or more of the constituents of the aluminum alloy in question.
  • an Al-Ba or Zn-Ba type alloy is suitable.
  • These intermetallic compounds or alloys can be obtained directly by reducing the barium oxide BaO with aluminum or zinc according to known methods.
  • the amounts of barium used are very small, that is to say less than 0.1% and even more preferably less than 0.05%. A value between 0.005% and 0.03% may be suitable.
  • the second embodiment is particularly advantageous when it is applied to an aluminum alloy which has a relatively high silicon content, for example of the order of 0.10%.
  • the metal barium is expensive.
  • the first embodiment uses a less expensive barium alloy, but leads to the increase of the silicon content and possibly iron in the aluminum alloy. However, it is surprising to note that this increase in the silicon content and possibly iron does not degrade the toughness or the resistance to fatigue. This is due to the fact that silicon and possibly iron are not incorporated in the same way: the morphology of the phases is significantly modified.
  • LT tenacity K app
  • Such a semi- finished product or structural element has a yield strength R p0.2 (L) greater than 600 MPa.
  • the product according to the invention is more resistant to exfoliation corrosion (EXCO test), determined on test pieces taken at mid-thickness, than a corresponding product without barium.
  • EXCO test exfoliation corrosion
  • the product according to the invention can have many possible uses, and it is particularly advantageous to use said product as a structural element in aircraft construction, and especially as an extrados wing element, as part of lower sails, as a sail-skin element, as a stiffener, as a spar, as a rib or as an element for bulkheads.
  • the method according to the invention has several advantages.
  • the mode of introduction of barium according to the invention avoids the use of hydrides, which increase the residual hydrogen content, may cause pores in the solidified metal.
  • Barium neutralizes the detrimental effect of residual silicon in aluminum-based structural hardening alloys, resulting in improved toughness, including K IC and K app .
  • Barium also improves resistance to corrosion, including exfoliating corrosion.
  • the section of the plates was of the order of 2150 x 450 mm.
  • the chemical composition, determined on a solid pion obtained from liquid metal taken from the casting channel, is shown in Table 1.
  • Table 1 Chemical Composition Sample Fe Yes Cu mg Zn Zr Ti Ba P4068 # 66 0.03 0.05 1.76 1.90 7.48 0.11 0.0230 - P4069-2 # 66 0.11 0.12 1.86 2.03 8.40 0.10 0.0200 0.0100
  • the alloy was refined with 0.8 kg / t AT5B and cast at 685 ° C with a speed of 65 mm / min in rolling plates. After cooling and scalping, the plates were homogenized at 463 ° C and hot rolled at 420 to 410 ° C. The sheets obtained were dissolved for 6 hours at 120 ° C. and then for 17 hours at 150 ° C. The end product was thus metallurgical T351.
  • the silicon content of the type 7449 aluminum alloy increases from 0.04% to 0.09% and that of Fe increases from 0.03% to 0.06%
  • the microstructure of the sample with added barium shows eutectic compounds "in the shape of sea urchins" ( figure 4 ) or "broccoli-shaped” (see figure 5 ).
  • the microstructure of the barium-free sample added reveals eutectic compounds in the form of platelets ( figure 6 ).
  • Exfoliation corrosion resistance (EXCO) results obtained on mid-thickness specimens show that the 7449 barium alloy (EXCO: EA performance) is more resistant to exfoliating corrosion than the barium-free reference product (performance EXCO: EB). The resistance to stress corrosion is also slightly improved.

Claims (11)

  1. Verfahren zur Herstellung von Kneterzeugnissen aus einer Legierung auf Aluminiumbasis vom Typ Al-Cu-Mg oder Al-Zn-Cu-Mg mit hoher Zähigkeit und hoher Ermüdungsfestigkeit, umfassend
    (a) die Herstellung einer flüssigen Aluminiumlegierung, welche zwischen 0,005 und 0,1 % Barium enthält, wobei Barium (aa) in metallischer Form oder (ab) in Form einer intermetallischen Verbindung oder Legierung mit einem oder mehreren Bestandteilen der genannten Aluminiumlegierung oder mit Silicium und/oder Eisen eingebracht wird,
    (b) das Vergießen der flüssigen Legierung zu einer Rohform (wie einem Pressbarren, Schmiedebarren oder Walzbarren),
    (c) die Warmumformung der Rohform,
    bei dem die flüssige Legierung auf Aluminiumbasis zwischen 3,5 und 5,5 % Kupfer, zwischen 1 und 2 % Magnesium, einen Eisenanteil kleiner als 0,30 %, einen Siliciumanteil kleiner als 0,30 % und die anderen Legierungs- und Verunreinigungselemente bis insgesamt 3 % enthält, wenn es sich um eine Legierung vom Typ Al-Cu-Mg handelt, und zwischen 4 und 14 % Zink, zwischen 1 und 3 % Kupfer, zwischen 1 und 3 % Magnesium, einen Eisenanteil kleiner als 0,30 %, einen Siliciumanteil kleiner als 0,30 % und die anderen Legierungs- und Verunreinigungselemente bis insgesamt 2 % enthält, wenn es sich um eine Legierung vom Typ Al-Zn-Cu-Mg handelt.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der Bariumgehalt des Kneterzeugnisses zwischen 0,005 und 0,03 % liegt.
  3. Verfahren nach den Ansprüchen 1 oder 2, bei dem Barium in Form einer intermetallischen Verbindung oder Legierung mit Aluminium und Zink eingebracht wird.
  4. Verfahren nach den Ansprüchen 1 oder 2, bei dem Barium in Form einer Legierung vom Typ Si (70 %) - Ba (30 %) eingebracht wird.
  5. Verfahren zur Herstellung von Kneterzeugnissen aus einer Legierung auf Aluminiumbasis vom Typ Al-Zn-Cu-Mg nach irgendeinem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die flüssige Legierung auf Aluminiumbasis zwischen 7 und 10,5 % Zink, zwischen 1,4 und 2,5 % Kupfer und zwischen 1,7 und 2,8 % Magnesium enthält.
  6. Verfahren zur Herstellung von Kneterzeugnissen aus einer Legierung auf Aluminiumbasis vom Typ Al-Zn-Cu-Mg nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass die flüssige Legierung auf Aluminiumbasis, der Barium zugemischt wird, aus der Gruppe ausgewählt wird, bestehend aus den Legierungen 7010, 7050, 7055, 7056, 7150, 7040, 7075, 7175, 7475, 7049, 7149, 7249, 7349 und 7449.
  7. Verfahren zur Herstellung von Kneterzeugnissen aus einer Legierung auf Aluminiumbasis vom Typ Al-Cu-Mg nach irgendeinem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die flüssige Legierung auf Aluminiumbasis, der Barium zugemischt wird, aus der Gruppe ausgewählt wird, bestehend aus den Legierungen 2024, 2024A, 2124, 2224, 2324, 2424, 2524.
  8. Kneterzeugnis, herstellbar durch das Verfahren nach irgendeinem der Ansprüche 1 bis 7.
  9. Kneterzeugnis aus einer Legierung auf Aluminiumbasis vom Typ Al-Zn-Cu-Mg, herstellbar durch das Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass seine Zähigkeit Kapp(L-T), gemessen gemäß ASTM-Norm E 561 an einer in halber Dicke entnommenen CCT-Probe mit W = 406 mm und B = 6,35 mm, mehr als 86 MPa√m beträgt.
  10. Kneterzeugnis, herstellbar durch das Verfahren nach irgendeinem der Ansprüche 5 oder 6, dadurch gekennzeichnet, dass seine Dehngrenze Rp0,2(L) mehr als 600 MPa beträgt.
  11. Verwendung eines Kneterzeugnisses nach irgendeinem der Ansprüche 8 bis 10 als Strukturelement im Flugzeugbau, und insbesondere als Element für die Tragflügeloberseite, als Element für die Tragflügelunterseite, als Element für die Tragflügelaußenhaut, als Versteifer, als Holm, als Rippe oder als Element für Schottwände.
EP05778801A 2004-06-25 2005-06-22 Verfahren zur herstellung hochfester und ermüdungsfester aluminiumlegierungsprodukte Not-in-force EP1766102B1 (de)

Applications Claiming Priority (2)

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FR0406957A FR2872172B1 (fr) 2004-06-25 2004-06-25 Produits en alliage d'aluminium a haute tenacite et haute resistance a la fatigue
PCT/FR2005/001572 WO2006010817A1 (fr) 2004-06-25 2005-06-22 Procede de fabrication de produits en alliage d’aluminium a haute tenacite et haute resistance a la fatigue

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EP1766102A1 EP1766102A1 (de) 2007-03-28
EP1766102B1 true EP1766102B1 (de) 2008-12-10

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US (1) US20070243097A1 (de)
EP (1) EP1766102B1 (de)
CN (1) CN100564571C (de)
AT (1) ATE417136T1 (de)
BR (1) BRPI0512590A (de)
CA (1) CA2570618A1 (de)
DE (1) DE602005011619D1 (de)
FR (1) FR2872172B1 (de)
WO (1) WO2006010817A1 (de)

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CN107881369B (zh) * 2017-10-27 2020-06-30 大唐东北电力试验研究所有限公司 铝钙锑中间合金孕育剂及其制备方法
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RU2713526C1 (ru) * 2019-06-07 2020-02-05 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" Высокопрочный литейный алюминиевый сплав с добавкой кальция
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DE1255928B (de) * 1966-01-13 1967-12-07 Metallgesellschaft Ag Verfahren zur Erzielung eines langanhaltenden Veredelungseffektes in Aluminium-Silicium-Legierungen
US4711762A (en) * 1982-09-22 1987-12-08 Aluminum Company Of America Aluminum base alloys of the A1-Cu-Mg-Zn type
US4631172A (en) * 1984-05-08 1986-12-23 Nadagawa Corrosion Protecting Co., Ltd. Aluminum alloys for galvanic anode
JPS6196052A (ja) * 1984-05-08 1986-05-14 Nakagawa Boshoku Kogyo Kk 流電陽極用アルミニウム合金
CN86105578A (zh) * 1986-07-19 1988-02-24 江苏工学院 精炼变质熔剂
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RU2184167C2 (ru) * 2000-09-14 2002-06-27 Государственное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" Сплав на основе алюминия и изделие, выполненное из этого сплава

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CN100564571C (zh) 2009-12-02
DE602005011619D1 (de) 2009-01-22
EP1766102A1 (de) 2007-03-28
CN1977063A (zh) 2007-06-06
US20070243097A1 (en) 2007-10-18
CA2570618A1 (fr) 2006-02-02
BRPI0512590A (pt) 2008-03-25
FR2872172A1 (fr) 2005-12-30
FR2872172B1 (fr) 2007-04-27
ATE417136T1 (de) 2008-12-15
WO2006010817A1 (fr) 2006-02-02

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